Patent GB-711360-A (GB)
Title: Improvements in and relating to lubricating greases
IPC: C09K23/54
Filed: 1951-06-22
Abstract: A lubricating grease comprises a major proportion of a lubricating oil and a minor proportion of a cation-exchangeable inorganic colloid bearing at least 30 per cent. by weight of cationic surface-active radicals, at least 50 per cent. of which are in the form of a salt with an acid of phosphorus, sulphur or silicon.  The exchangeable cations of the colloid may be replaced by hydrogen ions, by treatment with an acid such as hydrochloric acid, before treating with a cationic surface active agent.  The inorganic colloid may be a natural or synthetic complex silicate such as bentonites, for example, montmorillonite, hectorite, beidellite, saponite and nontronite, sepiolite, biotite, attapulgite, vermiculite, zeolites such as edingtonite, chabazite, natrolite and mordenites; synthetic zeolites containing hydrogen, sodium, potassium, barium, magnesium or ammonium as the exchangeable cation; and synthetic clays such as magnesia-silica-sodium oxide, lime-silica-potassium oxide and barium oxide-silica-lithium oxide.  Surface-active agents with which the inorganic colloid is reacted may be quaternary ammonium salts or hydroxides, such as trimethyl dodecyl or trimethyl tetradecyl ammonium chlorides, triethyl hexadecylammonium chloride, triethyl octadecylammonium bromide, dimethyl dihexadecyl, dimethyl dioctadecyl, dimethyl cetyl lauryl, dimethyl lauryl stearyl, dimethyl diheptadecyl, or dimethyl octadecyl octadecenyl ammonium chlorides, and diethyl dioleyl ammonium chloride; octadecyl, hexadecyl, dioctadecyl, octadecenyl, heptadecyl and 10-ketolauryl ammonium acetates, heptadecyl ammonium propionate and 12-hydroxystearylammonium lactate; and amine salts of organic and inorganic acids such as acetic, propionic or hydrohalide acids, for example, tetradecylamine, octadecenylamine, methyl-octadecylamine, dioctadecylamine, dihexadecylamine and octyloctadecylamine hydrochlorides, and octadecylamine, ethylhexadecylamine, octadecylheptadecylamine and ditetradecylamine hydrobromides. Specified acids of phosphorus, sulphur and silicon are phosphorous, hypophosphorus, hypophosphoric, orthophosphoric, pyrophosphoric, trimetaphosphoric, tetrametaphosphoric and metaphosphoric acids, sodium dihydrogen phosphate and methyl dihydrogen phosphate; dilauryl, dicetyl, distearyl, lauryl cetyl, dimethyl and dibutyl hydrogen phosphates, stearyl and lauryl dihydrogen phosphates, tetradecane-1-phosphinic acid and 10-phenyldecane-1-phosphonic acid; sulphuric and sulphurous acids; stearyl hydrogen sulphonate, petroleum hydrogen sulphonate, methyl hydrogen sulphonate and heptadecyl hydrogen sulphonate; and metasilicic, orthosilicic and polysilicic acids and methyl hydrogen silicate.  Lubricating oils referred to are mineral oils and synthetic lubricants such as oxyalkylene polymers, silicone fluids, organic phosphates, polymerized olefins and esters of dicarboxylic acids; examples given are propylene oxide polymers, ethylene oxide-propylene oxide copolymers, trimethylene glycol polymers, ethylene glycol-trimethylene glycol copolymers, tricresyl, trioctyl, diphenylcresyl and diphenyl-octyl phosphates, di(2-ethylhexyl) sebacate, di(3-methylheptyl) adipate and polyvinyl caprylate.  In one example, 60 per cent. by weight (based on the weight of clay used) of dimethyldiheptadecyl-ammonium chloride is added with stirring to a 2 per cent. hydrosol of hectorite clay.  Sufficient phosphoric acid is added to convert all the amine radicals to the phosphate salt, which after washing and filtering to remove water is added to a mineral lubricating oil.  The mixture is heated to eliminate water and then milled with more oil to form a grease. In an alternative process salt formation is effected after the aminogel has been added to the lubricating oil.